FTIR study of iron and aluminium forms of zeolite MCM-58 showed that location of heteroatoms in this IFR structure depends on the type of heteroatom. The combination of the pyridine and CO adsorption allowed determination of the concentration of hydroxyls in the 12- and 5/6-rings. Both Fe and Al are gen- erating hydroxyls pointing towards either 12-ring or 5/6-rings but the former are located in positions giv- ing Si–OH–Fe hydroxyls pointing mainly to the 12-rings while the latter gives rise to the Si–OH–Al groups pointing primarily to the narrower 5- and 6-rings. (Al)MCM-58 undergoes only minor dehydroxylation associated with the acid sites even at tempera- tures as high as 700 ° C, which indicates unique stabilization of Al atoms in the IFR structure. In the case of (Fe)MCM-58, dehydroxylation is more extensive. Furthermore the OH located in the 5/6- rings dehydroxylate at lower temperatures than those in the 12-rings. The study also demonstrates that the concentration of the framework and extraframework iron atoms can be determined by a simple method based on pyridine adsorption followed by IR spectroscopy.